data_0530-2 _audit_creation_date 2019-06-18 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2018/3' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C17 H15 N O2' _chemical_formula_sum 'C17 H15 N O2' _chemical_formula_weight 265.30 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.6242(8) _cell_length_b 9.1882(4) _cell_length_c 17.3579(9) _cell_angle_alpha 90 _cell_angle_beta 93.571(4) _cell_angle_gamma 90 _cell_volume 2646.2(2) _cell_formula_units_Z 8 _cell_measurement_reflns_used 2758 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 29.2260 _cell_measurement_theta_min 2.7990 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.92541 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1120 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_unetI/netI 0.0313 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 5867 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 24.995 _diffrn_reflns_theta_max 24.995 _diffrn_reflns_theta_min 2.351 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2684 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -17.00 16.00 1.00 3.50 -- -11.59 37.00-150.00 33 2 \w -97.00 70.00 1.00 3.50 -- -11.59 0.00 150.00 167 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0348323000 _diffrn_orient_matrix_UB_12 0.0342973000 _diffrn_orient_matrix_UB_13 0.0172803000 _diffrn_orient_matrix_UB_21 -0.0240239000 _diffrn_orient_matrix_UB_22 0.0349191000 _diffrn_orient_matrix_UB_23 0.0268602000 _diffrn_orient_matrix_UB_31 0.0059584000 _diffrn_orient_matrix_UB_32 -0.0597432000 _diffrn_orient_matrix_UB_33 0.0256158000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1982 _reflns_number_total 2331 _reflns_odcompleteness_completeness 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.195 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.046 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 185 _refine_ls_number_reflns 2331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0399 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+2.1556P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0903 _refine_ls_wR_factor_ref 0.0960 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Ternary CH refined with riding coordinates: C8(H8), C9(H9), C7(H7) 2.b Secondary CH2 refined with riding coordinates: C16(H16A,H16B) 2.c Aromatic/amide H refined with riding coordinates: C6(H6), C2(H2), C3(H3), C15(H15), C12(H12), C4(H4), C5(H5), C14(H14), C13(H13) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O2 O 0.71984(6) 0.72072(12) 0.81444(6) 0.0209(3) Uani 1 1 d . . . . . O1 O 0.81866(7) 0.68548(13) 0.90508(7) 0.0299(3) Uani 1 1 d . . . . . N1 N 0.61832(8) 0.40215(15) 0.72208(8) 0.0166(3) Uani 1 1 d . . . . . C1 C 0.63754(9) 0.26228(17) 0.84022(9) 0.0161(3) Uani 1 1 d . . . . . C10 C 0.61381(9) 0.66612(17) 0.71573(9) 0.0176(4) Uani 1 1 d . . . . . C8 C 0.62922(9) 0.53478(17) 0.84542(9) 0.0165(4) Uani 1 1 d . . . . . H8 H 0.574583 0.519396 0.862010 0.020 Uiso 1 1 calc R . . . . C6 C 0.69714(10) 0.17178(17) 0.87323(9) 0.0191(4) Uani 1 1 d . . . . . H6 H 0.751125 0.195956 0.869809 0.023 Uiso 1 1 calc R . . . . C9 C 0.63446(9) 0.67633(17) 0.80060(9) 0.0180(4) Uani 1 1 d . . . . . H9 H 0.599787 0.749300 0.822962 0.022 Uiso 1 1 calc R . . . . C2 C 0.55722(9) 0.22339(17) 0.84566(9) 0.0185(4) Uani 1 1 d . . . . . H2 H 0.516760 0.282189 0.823085 0.022 Uiso 1 1 calc R . . . . C11 C 0.60956(9) 0.52954(17) 0.68003(9) 0.0165(4) Uani 1 1 d . . . . . C7 C 0.65755(9) 0.40302(17) 0.79969(9) 0.0163(4) Uani 1 1 d . . . . . H7 H 0.716028 0.409123 0.795914 0.020 Uiso 1 1 calc R . . . . C17 C 0.75059(10) 0.66044(17) 0.88079(9) 0.0212(4) Uani 1 1 d . . . . . C3 C 0.53685(10) 0.09836(18) 0.88422(9) 0.0216(4) Uani 1 1 d . . . . . H3 H 0.482912 0.074306 0.888077 0.026 Uiso 1 1 calc R . . . . C15 C 0.59961(10) 0.79123(18) 0.67187(10) 0.0232(4) Uani 1 1 d . . . . . H15 H 0.600850 0.881515 0.696134 0.028 Uiso 1 1 calc R . . . . C12 C 0.59177(9) 0.52275(18) 0.59991(9) 0.0201(4) Uani 1 1 d . . . . . H12 H 0.587918 0.432813 0.575376 0.024 Uiso 1 1 calc R . . . . C4 C 0.59664(10) 0.00869(17) 0.91717(9) 0.0219(4) Uani 1 1 d . . . . . H4 H 0.583016 -0.075568 0.943034 0.026 Uiso 1 1 calc R . . . . C5 C 0.67661(10) 0.04550(18) 0.91128(9) 0.0220(4) Uani 1 1 d . . . . . H5 H 0.716923 -0.014682 0.932935 0.026 Uiso 1 1 calc R . . . . C14 C 0.58369(10) 0.7837(2) 0.59282(10) 0.0272(4) Uani 1 1 d . . . . . H14 H 0.575567 0.868174 0.563833 0.033 Uiso 1 1 calc R . . . . C16 C 0.68824(10) 0.56422(18) 0.91446(9) 0.0209(4) Uani 1 1 d . . . . . H16A H 0.661944 0.613681 0.955387 0.025 Uiso 1 1 calc R . . . . H16B H 0.712144 0.474582 0.934576 0.025 Uiso 1 1 calc R . . . . C13 C 0.58001(10) 0.64853(19) 0.55746(10) 0.0248(4) Uani 1 1 d . . . . . H13 H 0.569447 0.642566 0.504306 0.030 Uiso 1 1 calc R . . . . H1 H 0.6302(11) 0.326(2) 0.6942(11) 0.026(5) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O2 0.0210(6) 0.0215(6) 0.0200(6) 0.0031(5) -0.0001(5) -0.0052(5) O1 0.0258(7) 0.0310(7) 0.0317(7) 0.0040(6) -0.0067(5) -0.0110(5) N1 0.0189(7) 0.0176(7) 0.0133(7) -0.0015(6) 0.0007(5) 0.0007(6) C1 0.0171(8) 0.0189(8) 0.0125(8) -0.0034(7) 0.0010(6) -0.0010(6) C10 0.0134(8) 0.0216(9) 0.0182(8) 0.0017(7) 0.0039(6) 0.0038(6) C8 0.0143(8) 0.0204(8) 0.0150(8) 0.0001(7) 0.0031(6) -0.0020(6) C6 0.0167(8) 0.0220(8) 0.0188(8) -0.0018(7) 0.0014(7) 0.0012(6) C9 0.0150(8) 0.0193(8) 0.0199(9) -0.0018(7) 0.0030(7) 0.0004(6) C2 0.0170(8) 0.0198(8) 0.0183(8) -0.0013(7) -0.0015(6) 0.0006(6) C11 0.0092(7) 0.0228(9) 0.0178(8) 0.0018(7) 0.0037(6) 0.0016(6) C7 0.0136(8) 0.0204(8) 0.0147(8) 0.0002(7) 0.0007(6) -0.0015(6) C17 0.0258(10) 0.0187(8) 0.0188(9) -0.0009(7) -0.0002(7) -0.0027(7) C3 0.0198(9) 0.0220(9) 0.0229(9) -0.0018(7) 0.0009(7) -0.0055(7) C15 0.0251(9) 0.0215(9) 0.0235(9) 0.0007(8) 0.0067(7) 0.0090(7) C12 0.0165(8) 0.0272(9) 0.0168(8) -0.0016(7) 0.0026(6) 0.0038(7) C4 0.0317(10) 0.0160(8) 0.0179(9) 0.0000(7) 0.0016(7) -0.0044(7) C5 0.0273(9) 0.0198(9) 0.0182(9) -0.0014(7) -0.0035(7) 0.0045(7) C14 0.0296(10) 0.0302(10) 0.0224(9) 0.0085(8) 0.0067(7) 0.0150(8) C16 0.0253(9) 0.0211(9) 0.0162(8) -0.0007(7) 0.0018(7) -0.0031(7) C13 0.0208(9) 0.0382(10) 0.0155(8) 0.0030(8) 0.0026(7) 0.0105(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O2 C9 1.4819(18) . ? O2 C17 1.3494(19) . ? O1 C17 1.2049(19) . ? N1 C11 1.382(2) . ? N1 C7 1.460(2) . ? N1 H1 0.878(19) . ? C1 C6 1.389(2) . ? C1 C2 1.391(2) . ? C1 C7 1.519(2) . ? C10 C9 1.495(2) . ? C10 C11 1.399(2) . ? C10 C15 1.391(2) . ? C8 H8 0.9800 . ? C8 C9 1.521(2) . ? C8 C7 1.538(2) . ? C8 C16 1.525(2) . ? C6 H6 0.9300 . ? C6 C5 1.388(2) . ? C9 H9 0.9800 . ? C2 H2 0.9300 . ? C2 C3 1.382(2) . ? C11 C12 1.405(2) . ? C7 H7 0.9800 . ? C17 C16 1.508(2) . ? C3 H3 0.9300 . ? C3 C4 1.387(2) . ? C15 H15 0.9300 . ? C15 C14 1.383(2) . ? C12 H12 0.9300 . ? C12 C13 1.378(2) . ? C4 H4 0.9300 . ? C4 C5 1.382(2) . ? C5 H5 0.9300 . ? C14 H14 0.9300 . ? C14 C13 1.385(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C13 H13 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 O2 C9 109.48(12) . . ? C11 N1 C7 120.60(13) . . ? C11 N1 H1 113.6(12) . . ? C7 N1 H1 114.2(12) . . ? C6 C1 C2 118.76(15) . . ? C6 C1 C7 121.96(14) . . ? C2 C1 C7 119.27(14) . . ? C11 C10 C9 119.66(14) . . ? C15 C10 C9 120.56(15) . . ? C15 C10 C11 119.77(15) . . ? C9 C8 H8 110.9 . . ? C9 C8 C7 112.34(13) . . ? C9 C8 C16 101.29(12) . . ? C7 C8 H8 110.9 . . ? C16 C8 H8 110.9 . . ? C16 C8 C7 110.03(13) . . ? C1 C6 H6 119.8 . . ? C5 C6 C1 120.41(15) . . ? C5 C6 H6 119.8 . . ? O2 C9 C10 109.63(12) . . ? O2 C9 C8 103.73(12) . . ? O2 C9 H9 109.2 . . ? C10 C9 C8 115.70(13) . . ? C10 C9 H9 109.2 . . ? C8 C9 H9 109.2 . . ? C1 C2 H2 119.6 . . ? C3 C2 C1 120.76(15) . . ? C3 C2 H2 119.6 . . ? N1 C11 C10 121.65(14) . . ? N1 C11 C12 119.59(15) . . ? C10 C11 C12 118.68(15) . . ? N1 C7 C1 108.94(12) . . ? N1 C7 C8 110.31(13) . . ? N1 C7 H7 109.1 . . ? C1 C7 C8 110.38(12) . . ? C1 C7 H7 109.1 . . ? C8 C7 H7 109.1 . . ? O2 C17 C16 109.79(14) . . ? O1 C17 O2 121.18(15) . . ? O1 C17 C16 129.03(15) . . ? C2 C3 H3 119.9 . . ? C2 C3 C4 120.17(15) . . ? C4 C3 H3 119.9 . . ? C10 C15 H15 119.4 . . ? C14 C15 C10 121.16(16) . . ? C14 C15 H15 119.4 . . ? C11 C12 H12 119.8 . . ? C13 C12 C11 120.41(16) . . ? C13 C12 H12 119.8 . . ? C3 C4 H4 120.3 . . ? C5 C4 C3 119.49(15) . . ? C5 C4 H4 120.3 . . ? C6 C5 H5 119.8 . . ? C4 C5 C6 120.40(15) . . ? C4 C5 H5 119.8 . . ? C15 C14 H14 120.5 . . ? C15 C14 C13 118.99(16) . . ? C13 C14 H14 120.5 . . ? C8 C16 H16A 111.2 . . ? C8 C16 H16B 111.2 . . ? C17 C16 C8 102.92(13) . . ? C17 C16 H16A 111.2 . . ? C17 C16 H16B 111.2 . . ? H16A C16 H16B 109.1 . . ? C12 C13 C14 120.95(16) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 0 2 2216.61 12.01 0 0 -2 2211.94 11.94 0 0 -3 0.38 0.3 0 0 3 0.26 0.27 0 0 4 9999 36 0 0 -4 9944.08 35.82 0 0 -5 2.37 0.74 0 0 5 2.29 0.76 0 0 -6 280.35 7.39 0 0 6 287.77 7.67 0 0 -7 19.51 2.31 0 0 7 35.11 3.05 0 0 8 1564.38 20.8 0 0 -8 1573.1 20.34 0 0 9 6.66 1.75 0 0 -9 3.63 1.3 0 0 10 1671.41 24.3 0 0 -10 1707.83 24.02 0 0 -11 8.33 2.01 0 0 -12 163.03 8.34 0 0 13 51.97 5.26 0 0 -13 21.82 3.37 0 0 14 67.63 6.15 0 0 -14 26.24 3.84 0 0 15 44.02 5.5 0 0 -15 16.63 3.2 0 0 16 183.15 10.69 0 0 17 10.05 2.88 0 0 18 6.15 2.57 0 0 19 2.66 1.85 0 0 20 6.01 2.26 0 0 21 0.63 1.29 0 0 22 13.72 3.99 0 2 0 531.14 7.4 0 -2 0 525.8 7.22 0 2 -1 1901.47 11.53 0 -2 -1 1905.27 15.83 0 -2 1 1885.18 11.24 0 2 1 1878.21 15.95 0 -2 2 1088.82 10.21 0 2 2 1069.69 13.53 0 -2 -2 1106.65 13.44 0 -2 -3 4337.02 29.54 0 2 -3 4428.28 21.87 0 2 -4 38.63 2.28 0 -2 -4 39.13 3 0 2 -5 201.18 3.63 0 -2 -5 205.27 7.37 0 -2 5 194.01 3.54 0 -2 -6 1564.88 21.66 0 2 -6 1617.98 12.48 0 -2 6 1614.57 12.46 0 2 -7 551.64 8.45 0 -2 -7 553.81 13.64 0 2 7 529.3 13.57 0 -2 7 556.65 8.52 0 2 -8 14.6 1.56 0 -2 -8 12.76 2.15 0 -2 8 15.54 1.65 0 2 -9 12.44 1.6 0 -2 9 12.74 1.64 0 -2 -9 13.05 2.3 0 -2 -10 29.28 3.66 0 2 10 27.37 3.71 0 -2 10 22.2 2.31 0 2 -10 21.88 2.25 0 -2 -11 70.49 5.84 0 2 11 67.34 5.97 0 2 -11 69.07 4.25 0 -2 11 65.81 4.27 0 2 -12 27.81 2.93 0 -2 -12 28.72 3.85 0 -2 12 28.35 2.99 0 2 12 26.68 4 0 2 -13 2.81 1.31 0 2 13 1.54 1.13 0 -2 13 4.27 1.48 0 2 -14 34.21 3.66 0 2 14 36.31 4.95 0 2 15 50.68 5.99 0 2 -15 44.34 4.33 0 2 16 25.93 4.5 0 2 -16 30.05 3.77 0 -2 16 28.66 3.75 0 2 17 9.92 3.09 0 2 -17 6.17 2.02 0 -2 17 8.33 2.31 0 -2 18 38.98 4.78 0 2 18 42.44 6.14 0 -2 19 1.15 1.13 0 2 19 -0.87 1.35 0 2 20 1.74 1.54 0 2 21 3.43 2.57 0 2 22 29.19 6.2 0 2 23 2.69 2.17 0 -4 0 371 8.66 0 4 0 377.56 8.95 0 4 1 443.58 10.42 0 4 -1 426.22 8.77 0 -4 -1 433.59 10.11 0 -4 1 438.38 8.55 0 -4 2 0.91 0.43 0 4 2 2.25 0.99 0 4 -2 1.02 0.53 0 -4 -2 1.45 0.89 0 -4 3 576.92 7.28 0 -4 3 610.42 10.76 0 -4 -3 597.22 13.53 0 4 -3 562.56 7.87 0 4 3 545.57 13.29 0 -4 -4 1068.16 19.06 0 -4 4 1089.22 14.83 0 4 4 1052.93 19.32 0 -4 -5 108.15 6.38 0 4 5 113.88 6.67 0 4 -6 414.99 9.38 0 4 6 413.42 13.25 0 -4 -6 415.88 13.07 0 -4 -7 18.07 2.92 0 4 7 14.11 2.6 0 4 -7 17.67 2.06 0 -4 -8 242.81 10.9 0 4 8 242.71 11.18 0 4 -8 244.78 8.14 0 4 9 2.48 1.42 0 -4 -9 2.6 1.23 0 4 -9 3.8 1.19 0 4 10 34.65 4.65 0 4 -10 33.17 3.35 0 4 11 403.53 16.21 0 4 -11 407 12.18 0 -4 12 1256.56 13.31 0 4 -12 1306.31 23.02 0 4 12 1324.84 30.3 0 4 -13 652.88 10.67 0 4 -13 628.4 16.81 0 4 13 640.09 21.7 0 -4 13 677.64 11.01 0 4 -14 68.16 5.81 0 -4 14 74.98 4.02 0 4 -14 70.6 3.87 0 4 14 81.52 8.08 0 -4 15 31.33 2.86 0 4 -15 34.31 4.33 0 4 -15 31.97 2.82 0 4 15 28.51 4.96 0 -4 16 156.11 6.67 0 4 16 151.47 11.81 0 4 17 20.36 4.55 0 4 18 75.09 8.96 0 4 19 9.46 3.43 0 4 20 6.69 3.09 0 4 21 34.73 6.61 0 -6 0 79.06 4.94 0 6 0 75.17 5.05 0 -6 -1 699.36 15.6 0 6 1 719.4 16.27 0 6 -1 725.33 14.59 0 -6 1 703.73 13.6 0 -6 -2 114.96 6.62 0 6 2 98.89 6.36 0 -6 2 104.76 4.89 0 6 -2 109.38 5.29 0 6 3 8.6 2.27 0 -6 3 14.07 2.2 0 6 -3 10.63 1.6 0 -6 3 11.37 1.56 0 -6 -3 7.95 1.95 0 6 -4 57.33 3.07 0 6 4 55.37 5.29 0 -6 -4 64.71 5.45 0 -6 4 59.69 4.21 0 -6 4 60.08 2.89 0 -6 5 25.56 2.77 0 6 -5 21.86 1.3 0 -6 5 25.58 1.41 0 -6 -5 30.08 3.91 0 6 5 21.25 3.37 0 -6 -6 133.18 8.37 0 6 6 128.9 8.55 0 6 7 3.2 1.8 0 6 8 15.98 3.4 0 6 9 229.62 12.66 0 6 10 26.21 4.54 0 6 11 2.33 1.62 0 6 -12 55.01 4.71 0 6 12 49.28 6.67 0 6 13 29.07 5.19 0 6 -13 26.12 3.39 0 6 14 1.04 1.65 0 6 15 101.54 10.39 0 6 16 42.75 6.9 0 6 17 11.39 3.33 0 6 18 1.66 2.34 0 -8 0 67.56 5.35 0 8 0 73.72 5.91 0 -8 1 643.49 15.52 0 -8 -1 643.1 17.23 0 8 -1 662.66 16.77 0 8 1 643.12 18.02 0 -8 2 1.19 1.11 0 8 2 -0.74 0.91 0 -8 2 2.16 1.13 0 -8 -2 1.52 1.26 0 8 -2 0.3 0.77 0 8 -3 32.11 3.27 0 -8 3 27.58 2.75 0 -8 -3 31.04 4.2 0 8 3 26.59 4.14 0 8 -4 21.67 2.42 0 -8 4 20.53 2.14 0 8 4 24.73 4.01 0 -8 5 5.33 0.94 0 8 5 7.28 2.66 0 8 -5 5.29 0.94 0 8 6 42.16 5.51 0 8 7 13.27 3.21 0 8 8 8.71 3.11 0 8 9 59.93 7.28 0 8 10 113.87 10.3 0 8 11 9.27 3.24 0 8 12 11.13 3.77 0 8 13 0.4 1.88 0 8 14 -1.47 2.36 0 8 15 63.2 8.98 0 10 0 15.96 3.26 0 -10 1 2.56 1.07 0 10 1 3.73 1.7 0 10 -1 1.57 1.29 0 10 2 27.38 4.57 0 -10 2 28.79 4.01 0 10 -2 35.51 4.17 0 -10 3 9.83 2.39 0 10 3 7.89 2.49 0 -10 4 6.81 2.06 0 10 4 4.94 2.16 0 -10 5 11.62 2.45 0 10 5 17.7 4.35 0 10 6 8.54 3.01 0 10 7 89.5 9.37 0 10 8 1.34 1.75 0 10 9 1.24 1.55 0 10 10 94.74 10.47 0 10 11 50.15 7.9 0 10 12 2.39 2.5 0 12 6 22.25 5.33 0 12 7 23.34 5.62 0 12 8 17.72 5.14 -1 1 23 4.17 1.92 -1 1 22 12.34 3.96 -1 1 21 5.62 2.6 -1 -1 21 8.06 2.87 -1 -1 20 19.06 3.86 -1 1 20 22.78 4.75 -1 1 19 45.38 6.26 -1 -1 19 44.06 5.67 -1 -1 18 67.28 6.7 -1 1 18 75.39 7.69 -1 -1 17 17.78 3.35 -1 1 17 16.66 3.66 -1 -1 16 64.98 6.02 1 1 -16 56.03 5.5 -1 1 16 63.52 6.65 -1 -1 15 33.25 4.11 -1 1 15 21.71 3.81 1 1 -15 25.02 3.67 -1 1 14 61.11 5.97 1 -1 -14 65.65 6.11 -1 -1 14 53.49 4.97 1 1 -14 62.2 5.29 1 -1 -13 106.06 7.39 1 1 -13 101.84 6.49 -1 1 13 96.72 7.25 -1 1 12 89.46 6.62 1 1 -12 91.53 5.81 1 -1 -12 73.89 5.98 -1 -1 11 189.48 8.03 1 1 -11 208.17 8.29 -1 1 11 208.9 9.64 1 -1 -11 192.54 9.18 -1 -1 10 15.22 2.15 1 1 -10 12.65 1.92 1 -1 -10 16.76 2.62 1 1 -9 68.69 4.21 1 -1 -9 76.66 5.24 -1 1 8 605.95 14.09 1 1 -8 598.68 11.72 1 -1 -8 619.06 14.12 -1 -1 8 596.25 11.56 -1 1 7 2.02 0.83 1 -1 -7 3.04 1.05 1 1 -7 4.31 1 -1 -1 7 3.95 0.89 1 -1 -6 328.7 9.07 1 1 -6 291.37 6.86 -1 -1 6 319.48 7.12 -1 1 6 321.69 9.08 1 -1 -5 542.11 10.78 -1 -1 5 530.81 8.16 -1 1 5 526.16 10.73 1 1 -5 536.79 8.36 1 1 -4 1421.26 12.13 1 -1 -4 1372.52 15.84 -1 -1 4 1404.02 11.69 1 -1 -3 1.08 0.53 -1 -1 3 0.73 0.25 1 1 -3 0.52 0.27 1 -1 -2 1147 11.59 1 1 -2 1102.46 10.52 -1 -1 2 1117.9 8.49 1 1 -1 1.31 0.35 1 1 -1 0.54 0.19 -1 -1 1 0.36 0.18 1 1 0 1082.41 9.25 -1 -1 0 1070.44 9.23 1 -1 0 1064.85 8.08 -1 1 0 1059.54 7.94 -1 -1 -1 19.16 1.41 -1 -1 -2 1008.63 11.38 1 -1 3 37.34 1.55 -1 -1 -3 31.39 2.25 -1 1 -3 36.1 1.47 1 -1 4 25.72 1.55 -1 1 -4 25.9 1.51 -1 -1 -4 26.22 2.28 -1 -1 -5 472.72 10.31 -1 1 -5 475.29 7.48 1 1 5 482.91 10.55 1 -1 5 496.58 7.84 1 -1 6 207.05 5.69 -1 1 -6 198.67 5.45 -1 -1 -6 196.51 7.14 1 1 6 213.01 7.49 -1 -1 -7 1014.45 17.06 1 1 7 1009.3 17.35 1 -1 7 1015.56 13.95 -1 1 -7 1042.02 13.81 1 -1 8 12.06 1.73 1 1 8 13.93 2.19 -1 -1 -8 11.45 1.96 -1 1 -8 9.36 1.43 -1 1 -9 760.36 13.73 -1 -1 -9 784.09 16.71 1 -1 9 760.31 14.24 -1 -1 -10 23.61 3.09 -1 1 -10 21.78 2.51 1 -1 10 20.51 2.56 -1 -1 -11 156.9 8.25 1 1 11 157.83 8.46 -1 1 -11 156.04 7.09 1 -1 11 152.87 7.26 -1 1 -12 0.83 0.77 -1 -1 -12 1.41 1.02 1 1 12 0.03 0.75 1 1 13 106.8 7.63 -1 -1 -13 95.26 6.92 -1 1 -13 97.76 6.21 1 -1 14 -0.58 0.92 -1 -1 -14 -0.27 0.69 -1 1 -14 -0.27 0.9 1 1 14 0.48 1.25 -1 1 -15 26.37 3.61 1 1 15 32.04 4.72 1 -1 15 25.53 3.6 -1 1 -16 1.12 0.68 1 -1 16 0.36 0.99 1 1 16 1.36 1.37 1 1 17 7.53 2.69 -1 1 -17 8.15 2.3 1 -1 17 4.83 1.86 1 1 18 1.04 1.11 1 -1 18 -2.54 1.46 1 -1 19 30.5 4.82 1 1 19 32.16 5.37 1 -1 20 36.93 5.32 1 1 20 28.49 5.25 1 -1 21 77.52 7.99 1 1 21 53.81 7.48 1 1 22 29.27 5.91 1 1 23 57.74 8.24 -1 3 22 22.61 5.54 -1 3 21 2.81 2 -1 3 20 39.24 6.76 -1 3 19 0.38 1.18 -1 3 18 9.21 3.23 -1 -3 18 1.47 1.2 -1 3 17 21.7 4.53 1 3 -16 39.72 4.12 -1 3 16 36.32 5.57 1 3 -15 33.68 3.58 -1 3 15 24.89 4.46 -1 -3 15 26.73 3.18 1 3 -14 99.8 5.81 -1 -3 14 93.18 5.51 -1 3 14 101.19 8.56 -1 -3 13 428.25 11.03 -1 3 13 412.89 16.75 1 3 -13 440.05 11.44 1 3 -12 1350.13 18.72 -1 -3 12 1357.1 18.5 -1 3 12 1318.83 28.53 -1 3 11 1054.58 24.66 1 -3 -11 1072.92 24.33 -1 -3 11 1056.47 15.21 1 3 -11 1057.35 15.49 1 3 -10 394.57 8.73 -1 -3 10 392.86 8.54 -1 3 10 398.23 14.43 1 -3 -10 400.58 14.15 1 -3 -9 72.67 5.79 1 3 -9 68.59 3.35 -1 3 9 70.12 5.82 -1 -3 9 67.76 3.22 1 3 -8 35.43 2.2 -1 -3 8 33.5 2.02 1 3 -8 34.42 3.2 1 -3 -8 30.84 3.6 -1 -3 7 890.85 9.16 1 3 -7 910.57 15.47 -1 -3 6 136.48 3.35 -1 -3 6 148.38 3.29 1 -3 -6 149.48 7.28 -1 -3 5 535.51 5.93 1 3 -5 581.54 10.99 -1 3 5 565.46 13.57 -1 -3 5 533.73 6.26 1 -3 -5 579.42 13.46 1 3 -4 967.36 13.4 1 -3 -4 1005.53 16.7 -1 -3 4 939.68 8.42 -1 3 4 948.02 16.6 -1 -3 4 991.41 14.07 -1 -3 4 941.4 8.49 1 -3 -3 113.23 5.27 -1 3 3 114.12 5.4 1 3 -3 111.57 3.24 -1 -3 3 114.08 4.62 -1 -3 3 113.7 3.18 1 -3 -2 1267.25 16.34 1 3 -2 1262.84 12.47 -1 -3 2 1262.53 11.93 -1 -3 2 1269.42 14.81 -1 3 2 1268.85 16.67 -1 3 1 72.53 3.69 1 3 -1 74.84 3.39 1 -3 -1 75.68 3.69 -1 -3 1 76.71 3.28 1 -3 0 59.69 2.98 -1 -3 0 62.5 3.25 1 3 0 59.24 3.28 -1 3 0 56.48 2.92 -1 -3 -1 90.03 4.29 1 -3 1 90.94 3.25 1 3 1 87.61 4.29 -1 3 -1 93.83 3.3 1 -3 2 980.28 8.85 1 3 2 1008.45 15.44 -1 3 -2 967.8 8.86 -1 -3 -2 955.04 14.92 1 -3 3 27.06 1.72 -1 -3 -3 28.61 2.75 1 3 3 28.49 2.84 -1 -3 -4 1542.99 21.31 1 3 4 1545.47 21.74 1 3 5 1.45 0.89 -1 3 -5 0.74 0.45 -1 -3 -5 1.53 0.55 -1 -3 -6 122.51 6.67 -1 3 -6 111.4 4.26 -1 3 -7 0.38 0.32 -1 -3 -7 1.41 0.99 1 -3 8 1020.58 10.01 -1 3 -8 1040.27 9.59 1 3 9 210.9 10.26 -1 -3 -9 209.52 9.93 1 -3 9 203.55 5.23 -1 3 -9 203.55 5 1 -3 10 273.21 6.87 -1 3 -10 267.02 6.45 1 3 10 259.72 11.77 -1 -3 -10 267.33 11.67 1 -3 11 4.96 1.04 1 3 11 5.87 2.16 -1 3 -11 7.74 1.24 -1 -3 -11 6.3 1.96 -1 3 -12 222.16 7.04 1 3 12 225.94 12.05 1 -3 12 227.43 7.48 1 -3 13 320.39 9.52 -1 3 -13 308.21 8.92 1 3 13 290.31 14.23 1 -3 14 265.97 9.26 -1 3 -14 273.48 8.99 1 3 14 256.28 13.75 1 3 15 142.36 10.58 -1 3 -15 157.03 7.23 1 -3 15 165.67 7.73 -1 3 -16 3.49 1.13 1 3 16 3.02 1.84 1 3 17 1.68 1.7 1 -3 18 4.58 1.72 1 3 18 4.64 2.13 1 3 19 69.88 8.58 1 3 20 55.38 7.89 1 3 21 150.16 13.34 1 3 22 -2.18 1.97 -1 5 20 -2.6 2.6 -1 5 19 10.81 3.9 -1 5 18 11.12 3.83 -1 5 17 11.24 3.6 -1 5 16 234.89 15.2 -1 5 15 9.83 3.1 1 5 -14 100.76 7.21 -1 5 14 107.16 9.67 -1 5 13 147.19 10.91 1 5 -13 150.57 8.46 1 5 -12 149.17 8.05 -1 5 12 154.66 10.9 1 5 -11 38.28 4 -1 5 11 42.7 5.65 1 5 -10 6.27 1.6 -1 5 10 10.23 2.71 -1 5 9 39.27 5.04 1 5 -9 32.88 3.4 1 5 -8 18.34 2.46 -1 5 8 20.37 3.5 1 -5 -8 15.27 2.95 1 -5 -7 36.59 4.32 -1 5 7 39.12 4.6 1 -5 -6 45.8 4.61 -1 5 6 39.91 4.44 -1 5 5 1.04 0.81 -1 -5 5 0.62 0.32 -1 -5 5 1.24 0.71 1 -5 -5 1.94 0.9 1 -5 -4 54.82 4.62 -1 -5 4 50.35 2.53 -1 -5 4 54.76 3.97 -1 5 4 57.53 4.89 1 5 -4 54.47 2.82 -1 -5 3 89.76 3.84 1 -5 -3 89.47 5.62 -1 -5 3 93.21 5.05 1 5 -3 90.08 4.13 -1 5 3 84.35 5.59 1 -5 -2 108 5.85 -1 5 2 105.14 5.98 1 5 -2 111.68 5.02 -1 -5 2 101.5 4.54 1 -5 -1 83.96 4.88 -1 -5 1 82.06 4.42 1 5 -1 84.54 4.7 -1 5 1 77.45 4.84 1 5 0 89.74 5.15 1 -5 0 91.7 4.75 -1 -5 0 93.98 5.04 -1 5 0 94.31 4.98 1 5 1 12.68 2.04 -1 5 -1 11.49 1.61 -1 -5 -1 10.97 1.84 1 -5 1 16.03 1.88 -1 -5 -2 47.43 4.01 1 5 2 54.55 4.45 1 -5 2 45.78 2.86 -1 5 -2 48.12 2.98 1 -5 3 0.58 0.4 -1 5 -3 0.72 0.43 1 -5 3 0.36 0.31 1 5 3 0.84 0.81 -1 -5 -3 1.23 0.9 1 -5 4 100.55 4.52 -1 -5 -4 94.7 6.28 1 -5 4 95.03 2.84 -1 5 -4 87.7 2.81 1 5 4 86.63 6.16 1 5 5 354.91 12.89 -1 -5 -5 334.21 12.28 -1 -5 -6 125.89 7.81 1 5 6 109.95 7.53 1 5 7 18.55 3.21 -1 -5 -7 20.73 3.35 1 5 8 17.25 3.41 -1 -5 -8 20.01 3.38 -1 5 -9 6.04 1.26 1 5 9 7.33 2.32 -1 5 -10 2.99 1.09 1 5 10 3.55 1.96 -1 5 -11 131.03 6.45 1 5 11 131.91 9.82 1 5 12 24.6 4.51 -1 5 -12 21.98 2.89 1 5 13 58.41 7.02 -1 5 -13 72.51 5.34 -1 5 -14 6.2 2.03 1 5 14 6.63 2.79 1 5 15 119.28 10.6 -1 5 -15 106.99 7.14 1 5 16 4.05 2.32 1 5 17 0.66 1.92 1 5 18 4.14 2.52 1 5 19 -0.84 1.6 1 5 20 12.83 4.4 -1 7 17 226.02 16.82 -1 7 16 4.45 2.39 -1 7 15 14.99 4.36 -1 7 14 0.86 1.28 -1 7 13 18.76 4.56 -1 7 12 52.49 7.15 -1 7 11 25.91 5.06 -1 7 10 230.88 13.89 -1 7 9 9.52 3.17 -1 7 8 14.06 3.36 -1 7 7 104.03 8.49 -1 7 6 104.27 8.15 1 -7 -5 65.98 6.16 1 7 -5 63.06 3.26 -1 7 5 70.46 6.53 -1 -7 5 64.24 3.1 -1 7 4 95.74 7.25 -1 -7 4 98.56 4.45 1 -7 -4 103.22 7.36 1 7 -4 93.55 4.71 -1 -7 3 143.32 5.97 1 7 -3 146.84 6.6 -1 7 3 138.91 8.39 1 -7 -3 128.05 7.86 -1 -7 2 245.61 8.46 1 7 -2 257.49 9.31 -1 7 2 234.84 10.49 1 -7 -2 249.76 10.47 -1 7 1 514.78 14.69 1 -7 -1 518.34 14.31 1 7 -1 538.8 14.28 -1 -7 1 538.08 13.43 -1 7 0 127.82 6.98 1 7 0 119.32 7.09 1 -7 0 118.94 6.51 -1 -7 0 127.33 6.93 -1 7 -1 359.08 11.12 1 7 1 339.94 12.45 1 -7 1 342.83 10.5 -1 -7 -1 338.11 11.92 1 -7 2 165.07 6.69 -1 7 -2 167.26 7.08 1 7 2 168.73 9.1 -1 -7 -2 170.34 8.85 1 7 3 12.09 2.6 1 -7 3 8.37 1.38 1 -7 3 5.97 1.42 -1 7 -3 7.27 1.38 -1 -7 -3 10.14 2.24 -1 7 -4 13.24 1.63 1 7 4 11.07 2.64 -1 -7 -4 14.1 2.89 1 -7 4 11.69 2.02 1 -7 4 16.1 1.67 1 -7 5 36.72 1.86 1 7 5 48.51 5.5 1 -7 5 42.82 3.61 1 7 6 24.43 4.05 1 7 7 1.22 0.99 1 7 8 29.25 4.71 1 7 9 10.79 3.11 1 7 10 124.66 10.26 1 7 11 2.39 1.75 1 7 12 27.38 5.18 1 7 13 6.44 3.03 1 7 14 56.88 7.82 1 7 15 4.37 2.82 1 7 16 16.83 4.73 1 7 17 1.12 2.09 -1 9 14 8.14 3.51 -1 9 13 35.94 6.56 -1 9 12 32.36 6.31 -1 9 11 8.21 3.35 -1 9 10 13.32 3.74 -1 9 9 -0.58 2.05 -1 9 8 0.74 1.2 -1 9 7 43.88 6.06 -1 9 6 19.74 3.96 -1 -9 6 22.44 3.45 -1 -9 5 13.57 2.58 1 9 -5 9.33 1.49 -1 9 5 8.63 2.83 1 9 -4 166.14 7.27 -1 -9 4 167.35 9.23 -1 9 4 166.56 10.82 1 9 -3 2.3 1.24 -1 -9 3 2.62 1.47 -1 9 3 -0.65 1.05 -1 -9 2 4.67 1.93 -1 9 2 3.9 1.86 1 9 -2 3.72 1.57 1 9 -1 2.13 1.37 1 -9 -1 -0.1 0.82 -1 9 1 -1.23 1.34 -1 -9 1 -0.88 1.25 1 -9 0 92.3 6.61 -1 -9 0 105.62 7.24 -1 9 0 99.07 7.22 1 9 0 103.03 7.54 1 9 1 137.12 9.11 1 -9 1 131.15 7.43 -1 9 -1 139.23 8.1 -1 -9 -1 139.78 8.67 -1 9 -2 0.69 1.07 1 9 2 0.47 1.16 1 -9 2 1.03 1.16 1 9 3 2.75 1.44 -1 9 -3 4.02 1.3 1 -9 3 2.34 1.33 1 9 4 10.14 2.82 -1 9 -4 7.41 1.53 1 -9 4 10.65 2.29 1 9 5 9.75 2.75 1 9 6 35.67 5.49 1 9 7 99.22 9.49 1 9 8 55.93 7.25 1 9 9 4.98 2.84 1 9 10 17.95 4.64 1 9 11 94.55 10.33 1 9 12 5.6 3.07 1 9 13 0.11 1.41 -1 11 10 17.88 4.79 -1 11 9 2.4 2.29 -1 11 8 6.67 3.13 -1 11 7 20.37 4.81 -1 11 6 2.31 2.18 -1 11 5 3.66 1.98 -1 11 4 4 1.6 -1 11 3 5.18 2.36 -1 -11 2 12.56 3.07 -1 11 2 17.67 3.88 -1 -11 1 6.4 2.33 1 -11 0 0.66 1.11 -1 -11 0 -1.38 1.37 1 11 1 14.48 3.51 1 11 2 72.47 7.72 1 11 3 2.75 2.1 1 11 4 84.89 8.87 1 11 5 183.1 13.43 1 11 6 8.39 3.37 1 11 7 0.87 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5.24 -19 5 -3 4.32 2.51 -19 5 -4 7.56 3.08 -19 5 -5 10.98 4.1 -19 5 -6 23.84 5.47 -19 7 1 0.63 2.1 -19 7 0 -1.21 2.71 -20 0 7 2.22 1.64 -20 0 6 29.56 6.17 -20 0 5 4.42 3.17 -20 0 4 158.83 14.05 -20 0 3 -0.07 2.18 -20 0 2 17.86 4.92 -20 0 1 3.92 2.82 -20 0 0 8.8 3.82 -20 0 -1 2.15 1.91 -20 0 -2 20.38 5.29 -20 0 -3 0.01 1.8 -20 0 -4 4.89 3.1 -20 0 -5 3.22 2.05 -20 -2 7 10.85 4.06 -20 -2 6 43.14 7.47 -20 2 6 30.87 6.5 -20 -2 5 12.1 4.4 -20 2 5 12.1 4.44 -20 -2 4 37.66 7.02 -20 2 4 39.15 7.05 -20 -2 3 26.74 5.86 -20 2 3 37.04 7.05 -20 -2 2 58.64 8.73 -20 2 2 47.25 7.63 -20 -2 1 32.49 7.04 -20 2 1 22.31 5.61 -20 -2 0 0.23 1.56 -20 2 0 0.69 1.71 -20 -2 -1 0.82 1.69 -20 2 -1 2.09 2.3 -20 2 -2 16 4.79 -20 -2 -2 17.01 4.47 -20 2 -3 39.78 7.19 -20 -2 -3 33.51 5.89 -20 -2 -4 -1.29 2.16 -20 2 -4 2.11 1.95 -20 2 -5 1.75 1.64 -20 -2 -5 -1.61 2.53 -20 2 -6 21.71 5.27 -20 -2 -6 16.64 4.1 -20 2 -7 64.93 9.23 -20 -2 -7 75.18 8.69 -20 2 -8 34.19 6.66 -20 -2 -8 28.85 5.43 -20 2 -9 104.78 11.85 -20 -2 -9 107.75 10.43 -20 4 4 7.68 3.38 -20 4 3 3.72 2.57 -20 4 2 1.58 1.99 -20 4 1 28.26 5.98 -20 -4 1 27.52 5.71 -20 -4 0 12.96 4.39 -20 4 0 8.1 3.41 -20 -4 -1 35.16 6.63 -20 4 -1 41.21 7.26 -20 4 -2 11.48 4 -20 -4 -2 3.78 2.85 -20 4 -3 57.65 8.34 -20 -4 -3 47.42 7.58 -20 -4 -4 7.15 3.15 -20 4 -4 11.34 3.81 -20 4 -5 1.68 2.62 -20 4 -6 15.05 4.46 -20 4 -7 49.93 7.74 -20 6 -1 10.34 3.96 -20 6 -2 1.03 2.13 -21 1 1 12.45 4.45 -21 1 0 24.78 5.93 -21 1 -1 4.6 3.05 -21 1 -2 14.9 4.5 -21 -1 -5 153.08 12.22 -21 -1 -6 5.1 2.69 -21 -3 -1 17.23 4.62 -21 3 -2 2.78 2.04 -21 -3 -2 -0.24 1.83 -21 3 -3 2.72 2.85 -21 -3 -3 7.27 3.46 -21 -3 -4 -0.01 2.72 -21 -3 -5 16.03 4.54 -22 -2 -4 1.6 2.27 _iucr_refine_instructions_details ; TITL 0530-2_a.res in C2/c 0530-2.res created by SHELXL-2018/3 at 19:39:01 on 18-Jun-2019 REM Old TITL 0530-2 in C2/c REM SHELXT solution in C2/c: R1 0.128, Rweak 0.297, Alpha 0.022 REM 0.874 for 176 systematic absences, Orientation as input REM Formula found by SHELXT: C17 N O2 CELL 0.71073 16.6242 9.1882 17.3579 90 93.571 90 ZERR 8 0.0008 0.0004 0.0009 0 0.004 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O UNIT 136 120 8 16 L.S. 20 PLAN 20 BOND $H list 4 fmap 2 53 acta OMIT -3 50 REM REM REM WGHT 0.036500 2.155600 FVAR 0.35060 O2 4 0.719843 0.720716 0.814441 11.00000 0.02095 0.02155 = 0.02005 0.00308 -0.00006 -0.00523 O1 4 0.818659 0.685475 0.905075 11.00000 0.02582 0.03101 = 0.03171 0.00400 -0.00670 -0.01101 N1 3 0.618321 0.402148 0.722080 11.00000 0.01893 0.01755 = 0.01329 -0.00154 0.00067 0.00070 C1 1 0.637542 0.262278 0.840222 11.00000 0.01706 0.01893 = 0.01246 -0.00340 0.00100 -0.00102 C10 1 0.613813 0.666122 0.715734 11.00000 0.01339 0.02164 = 0.01819 0.00170 0.00394 0.00382 C8 1 0.629218 0.534782 0.845422 11.00000 0.01431 0.02044 = 0.01501 0.00010 0.00307 -0.00196 AFIX 13 H8 2 0.574583 0.519396 0.862010 11.00000 -1.20000 AFIX 0 C6 1 0.697141 0.171779 0.873229 11.00000 0.01667 0.02198 = 0.01877 -0.00184 0.00137 0.00123 AFIX 43 H6 2 0.751125 0.195956 0.869809 11.00000 -1.20000 AFIX 0 C9 1 0.634465 0.676327 0.800602 11.00000 0.01504 0.01926 = 0.01994 -0.00176 0.00305 0.00044 AFIX 13 H9 2 0.599787 0.749300 0.822962 11.00000 -1.20000 AFIX 0 C2 1 0.557218 0.223391 0.845656 11.00000 0.01697 0.01978 = 0.01828 -0.00128 -0.00153 0.00061 AFIX 43 H2 2 0.516760 0.282189 0.823085 11.00000 -1.20000 AFIX 0 C11 1 0.609560 0.529540 0.680029 11.00000 0.00922 0.02275 = 0.01777 0.00175 0.00368 0.00161 C7 1 0.657552 0.403017 0.799694 11.00000 0.01358 0.02044 = 0.01473 0.00022 0.00071 -0.00152 AFIX 13 H7 2 0.716028 0.409123 0.795914 11.00000 -1.20000 AFIX 0 C17 1 0.750590 0.660438 0.880789 11.00000 0.02582 0.01870 = 0.01881 -0.00086 -0.00022 -0.00273 C3 1 0.536853 0.098357 0.884220 11.00000 0.01983 0.02201 = 0.02290 -0.00178 0.00093 -0.00555 AFIX 43 H3 2 0.482912 0.074306 0.888077 11.00000 -1.20000 AFIX 0 C15 1 0.599613 0.791226 0.671874 11.00000 0.02511 0.02150 = 0.02352 0.00074 0.00667 0.00903 AFIX 43 H15 2 0.600850 0.881515 0.696134 11.00000 -1.20000 AFIX 0 C12 1 0.591774 0.522749 0.599909 11.00000 0.01646 0.02717 = 0.01682 -0.00164 0.00260 0.00380 AFIX 43 H12 2 0.587918 0.432813 0.575376 11.00000 -1.20000 AFIX 0 C4 1 0.596639 0.008693 0.917170 11.00000 0.03170 0.01596 = 0.01790 0.00004 0.00157 -0.00442 AFIX 43 H4 2 0.583016 -0.075568 0.943034 11.00000 -1.20000 AFIX 0 C5 1 0.676609 0.045505 0.911278 11.00000 0.02734 0.01977 = 0.01817 -0.00144 -0.00346 0.00454 AFIX 43 H5 2 0.716923 -0.014682 0.932935 11.00000 -1.20000 AFIX 0 C14 1 0.583685 0.783728 0.592817 11.00000 0.02963 0.03018 = 0.02241 0.00853 0.00674 0.01503 AFIX 43 H14 2 0.575567 0.868174 0.563833 11.00000 -1.20000 AFIX 0 C16 1 0.688241 0.564224 0.914463 11.00000 0.02533 0.02109 = 0.01624 -0.00066 0.00180 -0.00308 AFIX 23 H16A 2 0.661944 0.613681 0.955387 11.00000 -1.20000 H16B 2 0.712144 0.474582 0.934576 11.00000 -1.20000 AFIX 0 C13 1 0.580008 0.648531 0.557460 11.00000 0.02081 0.03817 = 0.01553 0.00296 0.00259 0.01046 AFIX 43 H13 2 0.569447 0.642566 0.504306 11.00000 -1.20000 AFIX 0 H1 2 0.630245 0.326342 0.694209 11.00000 0.02627 HKLF 4 REM 0530-2_a.res in C2/c REM wR2 = 0.0960, GooF = S = 1.080, Restrained GooF = 1.080 for all data REM R1 = 0.0399 for 1982 Fo > 4sig(Fo) and 0.0489 for all 2331 data REM 185 parameters refined using 0 restraints END WGHT 0.0359 2.1470 REM Highest difference peak 0.195, deepest hole -0.225, 1-sigma level 0.046 Q1 1 0.6235 0.6055 0.8191 11.00000 0.05 0.20 Q2 1 0.6183 0.6654 0.7522 11.00000 0.05 0.16 Q3 1 0.6323 0.5982 0.6938 11.00000 0.05 0.15 Q4 1 0.6017 0.2674 0.8622 11.00000 0.05 0.15 Q5 1 0.4665 0.7343 0.5223 11.00000 0.05 0.15 Q6 1 0.6179 0.5228 0.6406 11.00000 0.05 0.15 Q7 1 0.7006 0.4932 0.9560 11.00000 0.05 0.15 Q8 1 0.6447 0.3211 0.8193 11.00000 0.05 0.14 Q9 1 0.6408 0.4738 0.8200 11.00000 0.05 0.14 Q10 1 0.5645 0.0847 0.9293 11.00000 0.05 0.14 Q11 1 0.6017 0.5989 0.7007 11.00000 0.05 0.14 Q12 1 0.7006 0.6545 0.9227 11.00000 0.05 0.14 Q13 1 0.5560 0.3952 0.5954 11.00000 0.05 0.13 Q14 1 0.5853 0.7123 0.7001 11.00000 0.05 0.13 Q15 1 0.6677 0.6473 0.9419 11.00000 0.05 0.13 Q16 1 0.7571 0.6493 0.7630 11.00000 0.05 0.13 Q17 1 0.6317 0.7207 0.6978 11.00000 0.05 0.13 Q18 1 0.6888 0.1431 0.9242 11.00000 0.05 0.13 Q19 1 0.6634 0.1966 0.8264 11.00000 0.05 0.13 Q20 1 0.5403 0.6169 0.4927 11.00000 0.05 0.13 REM The information below was added by Olex2. REM REM R1 = 0.0399 for 1982 Fo > 4sig(Fo) and 0.0489 for all 7300 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.20, deepest hole -0.22 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0489 REM R1_gt = 0.0399 REM wR_ref = 0.0960 REM GOOF = 1.080 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 7300 REM Reflections_gt = 1982 REM Parameters = n/a REM Hole = -0.22 REM Peak = 0.20 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.132 _oxdiff_exptl_absorpt_empirical_full_min 0.862